#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:22:40 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179813 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010954.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7010954
loop_
_publ_author_name
'Fang Qi'
'Thomas C. W. Mak'
'Zhou Zhong-Yuan'
'Yang Qing-Chuan'
'Liu Zhi'
'Yu Wen-Tao'
'Zhu Dao-Ben'
'Jiang Min-Hua'
_publ_section_title
;
 Syntheses and crystal structures of the molecular conductors
 Z[Pd(dmit)2]2{Z = (Me3NEt)+, (MeNEt3)+, (NEt4)+} and their precursors
 Z2[Pd(dmit)2]
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1377
_journal_page_last               1385
_journal_paper_doi               10.1039/b105854c
_journal_year                    2002
_chemical_formula_sum            'C22 H40 N2 Pd S10'
_chemical_formula_weight         759.56
_chemical_name_common            (NEt4)2[Pd(dmit)2]
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.805(2)
_cell_length_b                   13.477(3)
_cell_length_c                   21.458(4)
_cell_measurement_temperature    294(2)
_cell_volume                     3413.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22434
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6175
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         4216
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1089P)²+0.8320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1994
_reflns_number_gt                2128
_reflns_number_total             4216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105854c.txt
_cod_data_source_block           e42pd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3414.0(12)
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7010954
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.0000 0.0606(2) Uani 1 2 d S . .
S1 S 0.13854(14) -0.11957(12) 0.01374(7) 0.0720(4) Uani 1 1 d . . .
S2 S 0.07236(15) 0.09146(13) 0.08265(8) 0.0788(5) Uani 1 1 d . . .
S3 S 0.34260(14) -0.12090(12) 0.09838(7) 0.0704(4) Uani 1 1 d . . .
S4 S 0.28553(15) 0.06135(13) 0.15866(8) 0.0789(5) Uani 1 1 d . . .
S5 S 0.49500(15) -0.04492(17) 0.19891(9) 0.0867(5) Uani 1 1 d . . .
C1 C 0.2186(5) -0.0644(4) 0.0734(2) 0.0621(14) Uani 1 1 d . . .
C2 C 0.1905(5) 0.0218(5) 0.1010(3) 0.0664(15) Uani 1 1 d . . .
C3 C 0.3812(5) -0.0346(5) 0.1542(3) 0.0713(16) Uani 1 1 d . . .
N1 N 0.2500 0.2500 -0.0850(3) 0.0698(18) Uani 1 2 d SD . .
C4 C 0.2694(13) 0.1849(11) -0.0304(6) 0.123(7) Uiso 0.539(16) 1 d PD . 2
H4A H 0.2698 0.2272 0.0062 0.148 Uiso 0.539(16) 1 calc PR . 2
H4B H 0.2037 0.1420 -0.0267 0.148 Uiso 0.539(16) 1 calc PR . 2
C5 C 0.3699(8) 0.1212(8) -0.0266(5) 0.145(4) Uani 1 1 d D . .
H5A H 0.3199 0.1332 0.0079 0.217 Uiso 0.461(16) 1 calc PR . 1
H5B H 0.4462 0.1147 -0.0115 0.217 Uiso 0.461(16) 1 calc PR . 1
H5C H 0.3479 0.0612 -0.0474 0.217 Uiso 0.461(16) 1 calc PR . 1
H5D H 0.3690 0.0854 0.0121 0.217 Uiso 0.539(16) 1 calc PR . 2
H5E H 0.4369 0.1615 -0.0286 0.217 Uiso 0.539(16) 1 calc PR . 2
H5F H 0.3697 0.0752 -0.0607 0.217 Uiso 0.539(16) 1 calc PR . 2
C4' C 0.3634(9) 0.2073(10) -0.0718(7) 0.100(6) Uiso 0.461(16) 1 d PD . 1
H4C H 0.4111 0.2601 -0.0559 0.120 Uiso 0.461(16) 1 calc PR . 1
H4D H 0.3959 0.1857 -0.1111 0.120 Uiso 0.461(16) 1 calc PR . 1
C6 C 0.1544(9) 0.1867(9) -0.0995(6) 0.106(6) Uiso 0.572(15) 1 d PD . 1
H6A H 0.0935 0.2298 -0.1132 0.127 Uiso 0.572(15) 1 calc PR . 1
H6B H 0.1299 0.1572 -0.0605 0.127 Uiso 0.572(15) 1 calc PR . 1
C6' C 0.2350(15) 0.1922(10) -0.1430(5) 0.099(7) Uiso 0.428(15) 1 d PD . 2
H6C H 0.3100 0.1721 -0.1564 0.118 Uiso 0.428(15) 1 calc PR . 2
H6D H 0.2070 0.2382 -0.1742 0.118 Uiso 0.428(15) 1 calc PR . 2
C7 C 0.1625(8) 0.1031(7) -0.1466(4) 0.132(3) Uani 1 1 d D . .
H7A H 0.0887 0.0752 -0.1533 0.198 Uiso 0.572(15) 1 calc PR . 1
H7B H 0.2126 0.0526 -0.1311 0.198 Uiso 0.572(15) 1 calc PR . 1
H7C H 0.1915 0.1285 -0.1852 0.198 Uiso 0.572(15) 1 calc PR . 1
H7D H 0.0849 0.1216 -0.1401 0.198 Uiso 0.428(15) 1 calc PR . 2
H7E H 0.1852 0.0566 -0.1151 0.198 Uiso 0.428(15) 1 calc PR . 2
H7F H 0.1704 0.0731 -0.1869 0.198 Uiso 0.428(15) 1 calc PR . 2
N2 N 0.2500 -0.2500 -0.1859(2) 0.0524(14) Uani 1 2 d SD . .
C8 C 0.1493(7) -0.2249(5) -0.1471(4) 0.111(3) Uani 1 1 d D . .
H8A H 0.0875 -0.2060 -0.1745 0.133 Uiso 1 1 calc R . .
H8B H 0.1674 -0.1679 -0.1214 0.133 Uiso 1 1 calc R . .
C9 C 0.1091(6) -0.3104(5) -0.1047(3) 0.088(2) Uani 1 1 d D . .
H9A H 0.0438 -0.2895 -0.0815 0.131 Uiso 1 1 calc R . .
H9B H 0.1687 -0.3281 -0.0763 0.131 Uiso 1 1 calc R . .
H9C H 0.0898 -0.3669 -0.1298 0.131 Uiso 1 1 calc R . .
C10 C 0.2757(6) -0.1608(5) -0.2271(3) 0.097(2) Uani 1 1 d D . .
H10A H 0.2901 -0.1038 -0.2007 0.117 Uiso 1 1 calc R . .
H10B H 0.2091 -0.1461 -0.2520 0.117 Uiso 1 1 calc R . .
C11 C 0.3771(6) -0.1751(6) -0.2710(3) 0.100(2) Uani 1 1 d D . .
H11A H 0.3879 -0.1160 -0.2953 0.150 Uiso 1 1 calc R . .
H11B H 0.3628 -0.2301 -0.2982 0.150 Uiso 1 1 calc R . .
H11C H 0.4440 -0.1879 -0.2468 0.150 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Pd1 S1 180.00(12) 5 . ?
S1 Pd1 S2 90.71(6) 5 5 ?
S1 Pd1 S2 89.29(6) . 5 ?
S1 Pd1 S2 89.29(6) 5 . ?
S1 Pd1 S2 90.71(6) . . ?
S2 Pd1 S2 180.00(8) 5 . ?
C1 S1 Pd1 100.3(2) . . ?
C2 S2 Pd1 100.5(2) . . ?
C3 S3 C1 98.1(3) . . ?
C3 S4 C2 98.8(3) . . ?
C2 C1 S3 116.8(4) . . ?
C2 C1 S1 123.6(5) . . ?
S3 C1 S1 119.5(3) . . ?
C1 C2 S2 124.7(5) . . ?
C1 C2 S4 114.5(5) . . ?
S2 C2 S4 120.8(4) . . ?
S5 C3 S4 124.3(4) . . ?
S5 C3 S3 123.9(4) . . ?
S4 C3 S3 111.8(4) . . ?
C6 N1 C6 155.3(12) . 2 ?
C6 N1 C6' 54.3(8) . . ?
C6 N1 C6' 102.9(9) 2 . ?
C6 N1 C6' 102.9(9) . 2 ?
C6 N1 C6' 54.3(8) 2 2 ?
C6' N1 C6' 65.3(11) . 2 ?
C6 N1 C4 113.4(8) . 2 ?
C6 N1 C4 86.6(10) 2 2 ?
C6' N1 C4 163.5(9) . 2 ?
C6' N1 C4 111.9(9) 2 2 ?
C6 N1 C4 86.6(10) . . ?
C6 N1 C4 113.4(9) 2 . ?
C6' N1 C4 111.9(9) . . ?
C6' N1 C4 163.5(9) 2 . ?
C4 N1 C4 75.4(13) 2 . ?
C6 N1 C4' 121.0(8) . . ?
C6 N1 C4' 64.3(7) 2 . ?
C6' N1 C4' 93.7(10) . . ?
C6' N1 C4' 104.9(9) 2 . ?
C4 N1 C4' 102.6(9) 2 . ?
C4 N1 C4' 58.7(8) . . ?
C6 N1 C4' 64.3(7) . 2 ?
C6 N1 C4' 121.0(8) 2 2 ?
C6' N1 C4' 104.9(9) . 2 ?
C6' N1 C4' 93.7(10) 2 2 ?
C4 N1 C4' 58.7(8) 2 2 ?
C4 N1 C4' 102.6(9) . 2 ?
C4' N1 C4' 158.0(13) . 2 ?
C5 C4 N1 121.0(9) . . ?
C5 C4 C4 140.4(18) . 2 ?
N1 C4 C4 52.3(6) . 2 ?
C4 C5 C4' 58.3(8) . . ?
N1 C4' C5 117.8(9) . . ?
N1 C6 C7 122.1(9) . . ?
N1 C6' C7 122.8(9) . . ?
C6' C7 C6 53.0(8) . . ?
C8 N2 C8 112.2(8) 2_545 . ?
C8 N2 C10 107.7(4) 2_545 2_545 ?
C8 N2 C10 110.2(5) . 2_545 ?
C8 N2 C10 110.2(5) 2_545 . ?
C8 N2 C10 107.7(4) . . ?
C10 N2 C10 109.0(7) 2_545 . ?
N2 C8 C9 113.9(5) . . ?
N2 C10 C11 114.4(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 S1 2.3149(16) 5 ?
Pd1 S1 2.3149(16) . ?
Pd1 S2 2.3226(16) 5 ?
Pd1 S2 2.3226(16) . ?
S1 C1 1.757(6) . ?
S2 C2 1.726(6) . ?
S3 C3 1.731(7) . ?
S3 C1 1.735(6) . ?
S4 C3 1.720(7) . ?
S4 C2 1.754(6) . ?
S5 C3 1.656(7) . ?
C1 C2 1.345(8) . ?
N1 C6 1.449(8) . ?
N1 C6 1.449(8) 2 ?
N1 C6' 1.479(8) . ?
N1 C6' 1.479(8) 2 ?
N1 C4 1.482(9) 2 ?
N1 C4 1.482(9) . ?
N1 C4' 1.484(9) . ?
N1 C4' 1.484(9) 2 ?
C4 C5 1.467(9) . ?
C4 C4 1.81(3) 2 ?
C5 C4' 1.514(9) . ?
C6 C7 1.517(9) . ?
C6' C7 1.477(8) . ?
N2 C8 1.490(6) 2_545 ?
N2 C8 1.490(6) . ?
N2 C10 1.523(6) 2_545 ?
N2 C10 1.523(6) . ?
C8 C9 1.545(7) . ?
C10 C11 1.535(7) . ?
